Acne removal cream as well as preparation method and application thereof
A combination of rosemary, knotweed, ampelopsis leaf and rosehip fruit extracts prepared by gradient ethanol extraction for acne treatment cream solves the problems of single effect and skin irritation of existing acne treatment products, and achieves multi-target acne treatment, anti-inflammatory, antioxidant and anti-aging effects.
Patent Information
- Application Number
- CN202511263678.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-05
- Publication Date
- 2025-11-11
AI Technical Summary
Most existing acne treatment products rely on a single antibacterial ingredient, which has limited effectiveness and poor skin penetration. Long-term use can easily cause skin allergies and irritation, and it is difficult to solve acne problems from multiple angles such as antibacterial, anti-inflammatory and antioxidant.
A plant extract composition consisting of rosemary, Japanese knotweed, Ampelopsis japonica leaf and prickly pear fruit extracts was prepared by gradient ethanol extraction to form an acne cream. This mixture was added to the acne cream formula, along with propylene glycol, shea butter and other ingredients, to form an oil phase and an aqueous phase mixture. Ascorbic acid and other ingredients were also added to form the acne cream.
It has significant antibacterial, anti-inflammatory, and antioxidant properties, promotes skin wound healing, reduces acne scars, and has anti-aging and anti-photoaging effects. It is suitable for sensitive skin and has significant and safe acne-removing effects.
Smart Images

Figure CN120919012A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of cosmetic technology, and in particular to an acne cream, its preparation method, and its application. Background Technology
[0002] Acne, commonly known as pimples, is a chronic inflammatory skin disease of the hair follicles and sebaceous glands that commonly occurs during adolescence and mainly affects the face. Studies have found that over 95% of people experience acne to varying degrees. Acne is classified into three degrees and four grades based on the nature of the skin lesions: mild (Grade I), with only comedones; moderate (Grade II), with inflammatory papules; moderate (Grade III), with pustules; and severe (Grade IV), with nodules and cysts. Propionibacterium acnes is a major cause of acne. It resides in the hair follicles and sebaceous glands, hydrolyzing triglycerides through lipases to produce more free fatty acids, causing a non-specific inflammatory reaction in and around the hair follicles. Currently, topical or oral medications for acne treatment are highly effective, but the relapse and rebound rates are very high, accompanied by local and systemic side effects. Treatment for acne mainly includes topical medications, oral medications, and physical laser therapy. Topical treatments for acne primarily include the use of retinoids, such as apadaline, and antibiotics, such as benzoyl peroxide. However, retinoids are photodegradable, increasing skin sensitivity and worsening lesions; antibiotics have varying degrees of skin irritation, and prolonged use can lead to drug resistance and carries a risk of liver and kidney damage. Physical laser therapy uses specific wavelengths of laser light to kill Propionibacterium acnes, accelerating tissue repair and clearing lesions, but it cannot eliminate acne at its root. Therefore, developing highly effective, gentle, non-irritating, safe, and long-lasting acne treatment products using natural ingredients has become an urgent market demand.
[0003] Currently, many acne treatment products on the market with added plant-based compounds have mediocre effects, mainly due to the following issues: some products only add a single antibacterial ingredient (such as cymene), resulting in a limited effect and poor skin penetration, thus affecting the acne-removing effect; others add too many types of plant extracts, which, while synergistically enhancing the effect, inadvertently increase the burden on the skin, increasing the risk of side effects such as skin allergies, irritation, and redness, thus affecting the long-term use of the product. The proliferation of Propionibacterium acnes promotes the growth of other bacteria such as Staphylococcus aureus, accelerating inflammation. Inflammation, in turn, triggers oxidative stress in the skin, causing skin damage. Therefore, simply inhibiting bacteria is insufficient to achieve good acne treatment results; a multi-pronged approach, addressing antibacterial, anti-inflammatory, and antioxidant effects, is necessary to tackle this common acne problem. Summary of the Invention
[0004] The purpose of this invention is to provide an acne cream, its preparation method, and its application, in order to solve the problems existing in the prior art.
[0005] To achieve the above-mentioned objectives, the present invention provides the following technical solution:
[0006] This invention provides an acne cream composed of the following components in the indicated mass fractions: 5-10% propylene glycol, 2-8% jojoba seed oil, 1-10% shea butter, 1-10% hydrogenated polydecene, 1-7% cetearyl alcohol, 1-6% petrolatum, 1-5% polydimethylsiloxane, 0.1-1.5% lauric acid / myristic acid / palmitic acid / glyceryl stearate, 0.1-0.6% hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, 0.1-2% peanut alcohol, 0.1-2.5% sodium lauryl sulfate, 0.04-19% plant extract composition, 0.1-1% sodium hyaluronate, 0.1-0.9% phenoxyethanol, and ascorbic acid. 0.1–3.8%, behenol 0.1–4.5%, C20-22 alcohol phosphate 0.1–2.9%, polyisobutylene 0.1–10%, C20-22 alcohol 0.1–3.1%, cetearyl glucoside 0.1–5.2%, carnosine 0.1–5%, arachidonic acid glucoside 0.1–2.5%, PEG-7 trimethylolpropionic acid ether 0.01–0.3%, sorbitan isostearate 0.01–5.7%, sodium sulfate 0.01–3%, C12–16 alcohol 0.001–4.3%, fructose 0.01–1.9%, butylene glycol 0.01–5.6%, phosphatidylcholine 0.01–3.4%, ceramide NP 0.001–1.3%, polyglycerol-10 oleate 0.001–1.8%, sodium stearoyl glutamate 0.001–1.5%, glyceryl caprylate 0.0001–2.2%, p-hydroxyacetophenone 0.0001–0.6%, balance being water.
[0007] Optionally, the plant extract composition comprises the following components in parts by weight: 0.01-9 parts rosemary extract, 0.01-2 parts Polygonum cuspidatum extract, 0.01-3 parts Ampelopsis japonica leaf extract, and 0.01-5 parts Rosa rugosa fruit extract;
[0008] The method for preparing the rosemary extract includes: gradient extraction of rosemary with ethanol, wherein the ratio of rosemary to ethanol is 1:10-20 (g / mL); the gradient extraction is performed sequentially with ethanol at volume concentrations of 100%, 85%, and 70%.
[0009] The preparation method of the Polygonum cuspidatum extract includes: gradient extraction of Polygonum cuspidatum with ethanol, wherein the ratio of Polygonum cuspidatum to ethanol is 1:10-20 (g / mL); the gradient extraction is performed sequentially with ethanol at volume concentrations of 90%, 80%, and 70%.
[0010] The preparation method of the Aeonium phalloides leaf extract includes: gradient extraction of Aeonium phalloides leaves with ethanol, wherein the ratio of Aeonium phalloides leaves to ethanol is 1:10-20 (g / mL); the gradient extraction is performed sequentially with ethanol at volume concentrations of 95%, 85%, and 75%.
[0011] The preparation method of the prickly pear fruit extract includes: extracting the prickly pear fruit with ethanol, wherein the ratio of prickly pear fruit to ethanol is 1:10-15 (g / mL); the gradient extraction is performed sequentially with ethanol at volume concentrations of 50%, 35%, and 20%.
[0012] Optionally, the method for preparing the plant extract composition includes mixing and pulverizing rosemary, Japanese knotweed, Ampelopsis japonica leaves and Rosa rugosa fruit to obtain a mixture, and performing gradient extraction on the mixture to obtain the plant extract composition.
[0013] The mass ratio of rosemary, Japanese knotweed, Amaryllis leaves, and prickly pear fruit is 1:1:1:1.
[0014] Optionally, the gradient extraction includes: sequentially extracting the mixture with ethanol at volume concentrations of 95%, 80%, 65%, 50%, and 35%; the material-to-liquid ratio of the mixture to ethanol is 1:15–20 (g / mL).
[0015] This invention also provides a method for preparing the above-mentioned acne cream, characterized by comprising the following steps:
[0016] (1) Propylene glycol, jojoba seed oil, shea butter, hydrogenated polydecene, cetearyl alcohol, petrolatum, polydimethylsiloxane, lauric acid / myristic acid / palmitic acid / glyceryl stearate, hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, arachidonic acid, sodium lauryl sulfate, behenyl alcohol, C20-22 phosphate ester, polyisobutylene, C20-22 alcohol, cetearyl glucoside, arachidonic acid glucoside, PEG-7 trimethylolpropionic acid coco ether, sorbitan isostearate, sodium sulfate and C12-16 alcohol are mixed to obtain oil phase A;
[0017] (2) Sodium hyaluronate and water are mixed to obtain aqueous phase B;
[0018] (3) After mixing oil phase A and water phase B, add plant extract composition, ascorbic acid, carnosine, fructose, butylene glycol, phosphatidylcholine, ceramide NP, polyglycerol-10 oleate, sodium stearoyl glutamate, glyceryl caprylate, p-hydroxyacetophenone and phenoxyethanol and stir evenly to obtain acne cream.
[0019] Optionally, the mixing temperature in step (1) is 75-80°C and the time is 10-15 min.
[0020] Optionally, the mixing temperature in step (2) is 75–80°C.
[0021] Optionally, in step (3), the temperature for mixing oil phase A and water phase B is 75-80°C. After mixing evenly, the temperature is lowered to 45-50°C, and other components are added.
[0022] Optionally, the stirring speed in step (3) is 1000-1200 r and the stirring time is 10-15 min.
[0023] This invention also provides the application of the above-mentioned acne cream in the preparation of facial care, body care, hair care and oral care products.
[0024] Compared with the prior art, the present invention has the following beneficial effects:
[0025] This invention aims to provide an acne cream with a plant extract composition for acne removal, its preparation method, and its application. This acne cream can improve acne of varying degrees, while also eliminating skin inflammation, resulting in good acne-removing effects. The acne cream contains a natural plant extract composition with excellent antibacterial, anti-inflammatory, and antioxidant effects. The scientifically formulated combination of four plant extracts can exert a synergistic effect from multiple targets and angles, including antibacterial, anti-inflammatory, and antioxidant properties. While significantly improving acne removal efficacy, it also promotes the recovery of moderate to severe open acne lesions due to its significant promotion of skin wound healing; it significantly inhibits tyrosinase activity, reduces intracellular melanin production, and reduces pigmentation deposition, thus reducing acne scar residue. It effectively and quickly eliminates acne scars and repairs acne marks and pits in a short time. In addition to providing long-term skin conditioning, it also has anti-aging, anti-photoaging, and UV damage prevention effects. Attached Figure Description
[0026] Figure 1 A bar chart showing the results of cytotoxicity experiments on 25 groups of plant extracts. * P<0.05, ** P<0.01, vs. blank group;
[0027] Figure 2 Bar charts showing pimple count, percentage of red area, and skin color a* value;
[0028] Figure 3 This is a report on the acne-removing efficacy and sensitive skin testing of the acne cream prepared in Example 14;
[0029] Figure 4 The report on acute eye irritation and repeated skin irritation tests of the acne cream prepared in Example 14;
[0030] Figure 5 The physicochemical test report for the acne cream prepared in Example 14;
[0031] Figure 6 The pesticide residue test report for the acne cream prepared in Example 14;
[0032] Figure 7 The report shows the microbial and heavy metal testing results for the acne cream prepared in Example 14. Detailed Implementation
[0033] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention.
[0034] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Every smaller range between any stated value or intermediate value within a stated range, and any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.
[0035] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.
[0036] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be obvious to those skilled in the art. This application specification and embodiments are merely exemplary.
[0037] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.
[0038] All raw materials used in this invention can be obtained commercially or prepared using existing technologies.
[0039] This invention provides an acne cream composed of the following components in the indicated mass fractions: 5-10% propylene glycol, 2-8% jojoba seed oil, 1-10% shea butter, 1-10% hydrogenated polydecene, 1-7% cetearyl alcohol, 1-6% petrolatum, 1-5% polydimethylsiloxane, 0.1-1.5% lauric acid / myristic acid / palmitic acid / glyceryl stearate, 0.1-0.6% hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, 0.1-2% peanut alcohol, 0.1-2.5% sodium lauryl sulfate, 0.04-19% plant extract composition, 0.1-1% sodium hyaluronate, 0.1-0.9% phenoxyethanol, and ascorbic acid. 0.1–3.8%, behenol 0.1–4.5%, C20-22 alcohol phosphate 0.1–2.9%, polyisobutylene 0.1–10%, C20-22 alcohol 0.1–3.1%, cetearyl glucoside 0.1–5.2%, carnosine 0.1–5%, arachidonic acid glucoside 0.1–2.5%, PEG-7 trimethylolpropionic acid ether 0.01–0.3%, sorbitan isostearate 0.01–5.7%, sodium sulfate 0.01–3%, C12–16 alcohol 0.001–4.3%, fructose 0.01–1.9%, butylene glycol 0.01–5.6%, phosphatidylcholine 0.01–3.4%, ceramide NP 0.001–1.3%, polyglycerol-10 oleate 0.001–1.8%, sodium stearoyl glutamate 0.001–1.5%, glyceryl caprylate 0.0001–2.2%, p-hydroxyacetophenone 0.0001–0.6%, balance being water.
[0040] In this invention, the acne cream comprises 0.04% to 19% of a plant extract composition, for example, it can be 0.04%, 0.05%, 0.08%, 0.1%, 0.2%, 0.5%, 0.8%, 1%, 2%, 3%, 4.7%, 5%, 6%, 7%, 8%, 9%, 10%, 15%, or 19%.
[0041] In this invention, the plant extract composition comprises the following components in parts by weight: 0.01-9 parts of rosemary extract, 0.01-2 parts of Polygonum cuspidatum extract, 0.01-3 parts of Amyda sinensis leaf extract, and 0.01-5 parts of Rosa rugosa fruit extract.
[0042] The plant extract composition in this formula, which has acne-reducing effects, is composed of rosemary extract, knotweed extract, ampelopsis leaf extract, and rosehip fruit extract, mixed in the optimal ratio for acne-reducing efficacy. All four extracts have significant antibacterial, anti-inflammatory, and antioxidant effects. Three of them are edible and have not been reported to be used in acne-reducing products. The active ingredients in the formula are derived from natural plants, making it safe, gentle, and non-irritating, with significant effects. The combined formula has a better acne-reducing effect, eliminating or reducing acne of different degrees. It is non-irritating, suitable for sensitive skin, and achieves a synergistic effect.
[0043] The plant extract composition of the present invention includes 0.01 to 9 parts of rosemary extract, for example, 0.01 parts, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts or 9 parts, etc.;
[0044] The preparation method of the rosemary extract includes: gradient extraction of rosemary with ethanol, wherein the ratio of rosemary to ethanol is 1:10 to 20 (g / mL), for example, 1:10 (g / mL), 1:15 (g / mL), or 1:20 (g / mL), preferably 1:15 (g / mL); the gradient extraction is performed sequentially with ethanol of volume concentrations of 100%, 85%, and 70%; the extraction is performed by ultrasonic extraction or heating reflux, with each ultrasonic extraction having a power of 380W and a time of 60 min.
[0045] Rosemary (Salvia rosmarinus Spenn.) is a perennial herb belonging to the genus Rosmarinus in the Lamiaceae family. It is a common and widely used edible spice, as well as a plant used for both food and medicine. Rosemary extract is a natural edible antioxidant approved for use by the FDA in my country; it is also an FDA-approved food preservative in Europe and the United States. Rosemary extract has a wide range of applications in food, cosmetics, and pharmaceuticals. Literature reports that rosemary extract can inhibit the growth of Propionibacterium acnes, reduce the inflammatory response induced by Propionibacterium acnes, and has significant acne-reducing effects; it also has significant inhibitory effects on other skin fungi, such as Microsporum gypseum and Mucor erythrorhizon, and can be used for skin fungal infections. Rosemary extract not only reduces skin oxidative damage caused by free radicals through its antioxidant effects, but also effectively inhibits lipid oxidation on the skin surface, inhibiting key anti-aging targets such as elastase, collagenase, and hyaluronidase, thus possessing anti-aging effects. Rosemary extract has a significant inhibitory effect on UVB-induced skin inflammation, reducing UVB-induced epidermal thickening, pigmentation, and wrinkle formation. Its main active ingredient, rosmarinic acid, can also prevent wrinkles by inhibiting UV-induced angiogenesis. Rosemary extract significantly promotes the formation of early microfibrils and mature elastic fibers in NHDFs (nitroglycerin-deficient fibers), and significantly upregulates MFAP-4, fibrin-1, and elastin, thereby preventing or improving photoaging. Furthermore, rosemary extract and its main components, rosmarinic acid and rosmarinic acid, effectively inhibit UV-induced expression of matrix metalloproteinases in human skin fibroblasts and keratinocytes, preventing UV damage; it also promotes wound healing in various wounds.
[0046] The plant extract composition of the present invention includes 0.01 to 2 parts of Polygonum cuspidatum extract, for example, 0.01 parts, 0.05 parts, 0.1 parts, 0.2 parts, 0.4 parts, 0.5 parts, 1 part or 2 parts, etc.
[0047] The preparation method of the Polygonum cuspidatum extract includes: gradient extraction of Polygonum cuspidatum with ethanol, wherein the solid-liquid ratio of Polygonum cuspidatum to ethanol is 1:10-20 (g / mL), for example, 1:10 (g / mL), 1:15 (g / mL), or 1:20 (g / mL), preferably 1:10 (g / mL); the gradient extraction is performed sequentially with ethanol at volume concentrations of 90%, 80%, and 70%; the extraction is performed by ultrasonic extraction or heating reflux, with each ultrasonic extraction having a power of 380W and a time of 60min.
[0048] Polygonum cuspidatum Sieb. et Zucc., the dried rhizome of the Polygonum cuspidatum plant (family Polygonaceae), is a commonly used traditional Chinese medicine. Slightly bitter, it possesses properties such as dispersing blood stasis, relieving cough, reducing jaundice, and promoting diuresis. Its chemical components include quinones, stilbenesides, flavonoids, and phenylpropanoids. Modern pharmacological studies have shown that it exhibits antibacterial, anti-inflammatory, antiviral, anti-HIV, anti-lipid peroxidation, and antioxidant effects. Resveratrol, the main active ingredient in Polygonum cuspidatum, significantly inhibits the growth of Propionibacterium acnes and lipocytes, with a sustained antibacterial effect superior to benzoyl peroxide, making it suitable for treating acne. Human acne treatment experiments have shown that it can reduce acne by 53.7% and large-area comedones by 72.5%, demonstrating significant acne-reducing efficacy. Polygonum cuspidatum extract and its main active ingredients have significant tyrosinase inhibitory activity, inhibiting melanin production, reducing pigmentation, and whitening the skin. The extract can also restore skin-related phenotypes, enhance skin protection, significantly resist skin aging, and promote skin wound healing in a rat skin wound model by reducing ROS levels in the skin.
[0049] The plant extract composition of the present invention includes 0.01 to 3 parts of Amorphophallus praecox leaf extract, for example, 0.01 parts, 0.1 parts, 1 part, 2 parts or 3 parts, etc.
[0050] The preparation method of the *Ampelopsis grossedentata* leaf extract includes: gradient extraction of *Ampelopsis grossedentata* leaves with ethanol, wherein the ratio of *Ampelopsis grossedentata* leaves to ethanol is 1:10-20 (g / mL), for example, 1:10 (g / mL), 1:15 (g / mL), or 1:20 (g / mL), preferably 1:15 (g / mL); the gradient extraction is performed sequentially with ethanol at volume concentrations of 95%, 85%, and 75%; the extraction is performed by ultrasonic extraction or heating reflux, with each ultrasonic extraction using a power of 380W and a time of 60 minutes.
[0051] Ampelopsis grossedentata (Hand.-Mazz.) WT Wang, a vine belonging to the genus Ampelopsis in the family Vitaceae, is also known as vine tea. Vine tea has been a daily beverage for residents of Guangxi, Hunan, Guizhou, and other regions since ancient times, highly regarded for its unique taste and health benefits. Literature reports the isolation and identification of 57 compounds from vine tea, mainly including flavonoids, phenols, steroids, and terpenes. Modern pharmacological studies have shown that vine tea possesses anti-inflammatory, antibacterial, antioxidant, antitumor, hepatoprotective, and immune-enhancing effects, with no toxic side effects. Due to its various health benefits, such as reducing liver damage and alleviating hangovers, vine tea is widely used and developed into various dosage forms of health products. Its antioxidant properties also make it suitable as a food additive. The leaf extract of *Ampelopsis grossedentata* exhibits significant inhibition of tyrosinase activity, reducing intracellular melanin production and pigmentation, thus possessing whitening effects. It also lowers intracellular ROS levels, effectively alleviating oxidative stress in animal skin, preventing oxidative damage, and exhibiting anti-aging properties. A nano-ointment made from *Ampelopsis grossedentata* leaf extract can be used to promote skin wound healing.
[0052] The plant extract composition of the present invention includes 0.01 to 5 parts of prickly pear fruit extract, for example, 0.01 parts, 0.1 parts, 1 part, 2 parts, 3 parts, 4 parts or 5 parts, etc.
[0053] The preparation method of the prickly pear fruit extract includes: extracting the prickly pear fruit with ethanol, wherein the ratio of prickly pear fruit to ethanol is 1:10-15 (g / mL), for example, 1:10 (g / mL), 1:11 (g / mL), 1:12 (g / mL), 1:13 (g / mL), 1:14 (g / mL), or 1:15 (g / mL), preferably 1:15 (g / mL); the gradient extraction is performed sequentially with ethanol at volume concentrations of 50%, 35%, and 20%; the extraction is performed by ultrasonic extraction or heating reflux, with each ultrasonic extraction using a power of 380W and a time of 60 minutes.
[0054] Rosa roxburghii Tratt., the mature fruit of the Rosa genus in the Rosaceae family, is a plant used for both medicinal and culinary purposes. Rich in Vitamin C, superoxide dismutase (SOD), and rosa flavonoids, it is known as the "Three Kings Sacred Fruit" due to its excellent pharmacological effects, including antioxidant, antibacterial, anti-inflammatory, anti-aging, anti-stress, anti-fatigue, hypoxia-resistance, regulation of glucose and lipid metabolism, organ protection, digestive system regulation, and radiation protection. Rosa roxburghii fruit extract exhibits significant anti-skin aging effects both in vitro and in vivo, primarily by significantly reducing β-galactosidase activity, improving skin hydration, radiance, elasticity, SOD activity, and reducing MDA accumulation. It can also effectively reduce IL-8 overexpression caused by UV radiation damage, alleviate skin inflammation, inhibit the interaction between denatured U1 RNA in damage-associated molecular patterns (DAMs) released by UV-damaged cells and surrounding cells, and significantly alleviate sunburn. In terms of anti-photoaging, the fermented broth of prickly pear fruit can effectively protect human embryonic skin fibroblasts from UVA-induced oxidative stress, exhibiting a significant anti-photoaging effect. Furthermore, the main components of prickly pear, vitamin C and superoxide dismutase, can significantly inhibit melanin production and tyrosinase activity, reducing UV-induced melanin deposition in the mouse ear, thus having a skin whitening effect.
[0055] In this invention, the method for preparing the plant extract composition includes mixing and pulverizing rosemary, Japanese knotweed, Ampelopsis japonica leaves and Rosa rugosa fruit to obtain a mixture, and performing gradient extraction on the mixture to obtain the plant extract composition.
[0056] The mass ratio of rosemary, Japanese knotweed, Amaryllis leaves, and prickly pear fruit is 1:1:1:1.
[0057] In this invention, the gradient extraction includes: sequentially extracting the mixture with ethanol at volume concentrations of 95%, 80%, 65%, 50%, and 35%; the material-to-liquid ratio of the mixture to ethanol is 1:15 to 20 (g / mL), for example, 1:15 (g / mL), 1:16 (g / mL), 1:17 (g / mL), 1:18 (g / mL), 1:19 (g / mL), or 1:20 (g / mL); the extraction is performed by ultrasonic extraction or heating reflux, with each ultrasonic extraction using a power of 380W for 60 minutes.
[0058] The plant extract composition provided by this invention can also be used in other facial, body, hair and oral care products. The amount of the plant extract composition added to any facial, body, hair and oral care product, such as serum, face cream, body lotion, neck cream, hair care and oral care, accounts for 0.01% to 60% of the total mass of the product.
[0059] This invention also provides a method for preparing the above-mentioned acne cream, characterized by comprising the following steps:
[0060] (1) Mix propylene glycol, jojoba seed oil, shea butter, hydrogenated polydecene, cetearyl alcohol, petrolatum, polydimethylsiloxane, lauric acid / myristic acid / palmitic acid / glyceryl stearate, hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, arachidonic acid, sodium lauryl sulfate, behenol, C20-22 phosphate ester, polyisobutylene, C20-22 alcohol, cetearyl glucoside, arachidonic acid glucoside, PEG-7 trimethylolpropionic acid coco ether, sorbitan isostearate, sodium sulfate and C12-16 alcohol and heat, stirring until completely dissolved to obtain oil phase A;
[0061] (2) Sodium hyaluronate and distilled water are heated and mixed until completely dissolved to obtain aqueous phase B;
[0062] (3) After mixing oil phase A and aqueous phase B evenly, cool the mixture and then add the plant extract composition, ascorbic acid, carnosine, fructose, butylene glycol, phosphatidylcholine, ceramide NP, polyglycerol-10 oleate, sodium stearoyl glutamate, glyceryl caprylate, and p-hydroxyacetophenone. Stir until the mixture is evenly mixed.
[0063] (4) Add the preservative phenoxyethanol to (3), stir evenly, cool to 30°C, filter and discharge to obtain acne cream.
[0064] In this invention, the mixing temperature in step (1) is 75-80°C, preferably 80°C, and the time is 10-15 min, preferably 15 min.
[0065] In this invention, the mixing temperature in step (2) is 75-80°C, preferably 80°C.
[0066] In this invention, the temperature of mixing oil phase A and water phase B in step (3) is 75-80°C. After mixing evenly, the temperature is lowered to 45-50°C, and other components are added.
[0067] In this invention, the stirring speed in step (3) is 1000-1200 r, preferably 1200 r, and the time is 10 min; the stirring speed in step (4) is 1000-1200 r, preferably 1200 r, and the time is 5 min.
[0068] The present invention also provides the application of the above-mentioned acne cream in the preparation of facial care, body care, hair care and oral care products.
[0069] The facial care includes serums, face creams, etc.; the body care includes body lotions, neck creams, etc.; the hair care includes shampoos, conditioners, etc.; and the oral care includes toothpaste, mouthwash, etc.
[0070] The technical solutions provided by the present invention will be described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of protection of the present invention.
[0071] Preparation Example 1
[0072] (1) Take crushed dried rosemary leaves, mix 100g of rosemary with 1500mL of 100% ethanol, and extract under ultrasonic power of 380W for 60min; after extraction, separate solid and liquid, collect extract 1, mix the solid with 1500mL of 85% ethanol, and extract under ultrasonic power of 380W for 60min; after extraction, separate solid and liquid, collect extract 2, mix the solid with 1500mL of 70% ethanol, and extract under ultrasonic power of 380W for 60min; after extraction, separate solid and liquid, collect extract 3, mix extract 1, extract 2 and extract 3, concentrate under reduced pressure until dry to obtain rosemary extract;
[0073] (2) Take the crushed dried root of Polygonum cuspidatum, mix 100g of dried root of Polygonum cuspidatum with 1000mL of 90% ethanol, and extract under ultrasonic power of 380W for 60min; after extraction, separate the solid and liquid, collect extract 1, mix the solid with 1000mL of 80% ethanol, and extract under ultrasonic power of 380W for 60min; after extraction, separate the solid and liquid, collect extract 2, mix the solid with 1000mL of 70% ethanol, and extract under ultrasonic power of 380W for 60min; after extraction, separate the solid and liquid, collect extract 3, mix extract 1, extract 2 and extract 3, concentrate under reduced pressure until dry to obtain Polygonum cuspidatum extract;
[0074] (3) Take the crushed dried stems and leaves of Amaryllis macrantha. First, mix 100g of dried stems and leaves of Amaryllis macrantha with 1500mL of 95% ethanol and extract under ultrasonic power of 380W for 60min. After extraction, separate the solid and liquid, collect extract 1, mix the solid with 1500mL of 85% ethanol and extract under ultrasonic power of 380W for 60min. After extraction, separate the solid and liquid, collect extract 2, mix the solid with 1500mL of 75% ethanol and extract under ultrasonic power of 380W for 60min. After extraction, separate the solid and liquid, collect extract 3, mix extract 1, extract 2 and extract 3, concentrate under reduced pressure until dry to obtain Amaryllis macrantha leaf extract.
[0075] (4) Take crushed and dried prickly pear fruit, mix 100g of prickly pear fruit with 1500mL of 50% ethanol, and extract under ultrasonic power of 380W for 60min; after extraction, separate solid and liquid, collect extract 1, mix the solid with 1500mL of 35% ethanol, and extract under ultrasonic power of 380W for 60min; after extraction, separate solid and liquid, collect extract 2, mix the solid with 1500mL of 20% ethanol, and extract under ultrasonic power of 380W for 60min; after extraction, separate solid and liquid, collect extract 3, mix extract 1, extract 2 and extract 3, concentrate under reduced pressure until dry to obtain prickly pear fruit extract;
[0076] Test Example 1
[0077] The rosemary extract, Japanese knotweed extract, Amygdalus leaf extract, and Rosa rugosa fruit extract prepared in Preparation Example 1 were mixed according to a four-factor, five-level orthogonal experimental design and the proportions shown in Table 1 to obtain the plant extract composition.
[0078] Table 1. Composition of Plant Extracts
[0079]
[0080]
[0081] Experiments were conducted on the toxicity of each group of plant extract compositions in Table 1 to human skin epidermal cells.
[0082] (1) Experimental methods
[0083] Cell line: HaCaT normal human skin epidermal cells, purchased from the cell resource platform of Peking Union Medical College.
[0084] Cell culture: Cells were cultured in a constant temperature cell culture incubator at 37°C and 5% CO2 under the following conditions: high glucose DMEM complete culture medium containing 15% fetal bovine serum (containing 1% penicillin-streptomycin mixture).
[0085] MTT assay for cytotoxicity: 2 × 10⁻⁶ cells were added to a 96-well plate. 4 HaCaT cells in the logarithmic growth phase were cultured overnight in a 5% CO2 incubator at 37°C. For each experimental group, a sample at a concentration of 100 μg / mL or a blank control group was added, along with an equal volume of culture medium for 24 h. Each group was treated in triplicate. Four h before the end of the experiment, 20 μL of LMT was added to each well for continued culture. After the experiment, the culture medium was aspirated, and 20 μL of DMSO was added to each well. The mixture was shaken thoroughly, and the OD value was measured at 540 nm using a microplate reader after 10 min.
[0086] Cell viability (%) = mean of drug-treated group / blank group × 100%.
[0087] (2) Experimental Results
[0088] The results are as follows Figure 1 As shown, at a concentration of 100 μg / mL, the MTT assay was used to conduct human skin epidermal cell toxicity tests on 25 groups of plant extract compositions. The results are as follows. Figure 1 As shown, a certain degree of cytotoxicity was observed when the proportion of Polygonum cuspidatum extract exceeded 25%. Therefore, the proportion of Polygonum cuspidatum extract in the plant extract composition should be equal to or less than 25%. Thus, after excluding compositions with certain cytotoxicity and those with repetitive proportions, Table 1 shows 12 groups requiring further testing for antibacterial, anti-inflammatory, and antioxidant activities. These were: Rosemary extract: Polygonum cuspidatum extract: Acer palmatum leaf extract: Rosa rugosa fruit extract = 1:1:1:1, 1:3:5:7, 3:1:9:7, 3:5:7:9, 5:1:7:3, 5:3:1:9, 7:1:5:9, 7:3:9:5, 9:1:3:5, 9:3:7:1, 9:5:1:7, 9:7:5:3. The final activity experiment determined that the ratio of Rosemary extract: Polygonum cuspidatum extract: Acer palmatum leaf extract: Rosa rugosa fruit extract = 1:1:1:1 had the best activity.
[0089] Example 1
[0090] Take the four plant extracts prepared in Preparation Example 1, and take 1 part by weight of rosemary extract, 1 part of Polygonum cuspidatum extract, 1 part of Amygdalus leaf extract, and 1 part of Prickly pear fruit extract, and mix them to obtain the plant extract composition.
[0091] Example 2
[0092] Take the four plant extracts prepared in Preparation Example 1, and take 3 parts by weight of rosemary extract, 1 part of knotweed extract, 1 part of ampelopsis leaf extract, and 1 part of prickly pear fruit extract, and mix them to obtain the plant extract composition.
[0093] Example 3
[0094] Take the four plant extracts prepared in Preparation Example 1, and take 5 parts by weight of rosemary extract, 1 part of knotweed extract, 1 part of ampelopsis leaf extract, and 1 part of prickly pear fruit extract, and mix them to obtain the plant extract composition.
[0095] Example 4
[0096] Take the four plant extracts prepared in Preparation Example 1, and take 9 parts by weight of rosemary extract, 1 part of knotweed extract, 1 part of ampelopsis leaf extract, and 1 part of prickly pear fruit extract, and mix them to obtain the plant extract composition.
[0097] Example 5
[0098] Take the four plant extracts prepared in Preparation Example 1, and take 10 parts by weight of rosemary extract, 1 part of knotweed extract, 1 part of ampelopsis leaf extract, and 1 part of prickly pear fruit extract, and mix them to obtain the plant extract composition.
[0099] Example 6
[0100] Take the four plant extracts prepared in Preparation Example 1, and take 1 part of rosemary extract, 1 part of Polygonum cuspidatum extract, 2 parts of Amyda sinensis leaf extract, and 1 part of Rosa rugosa fruit extract by weight. Mix them well to obtain the plant extract composition.
[0101] Example 7
[0102] Take the four plant extracts prepared in Preparation Example 1, and take 1 part of rosemary extract, 1 part of Polygonum cuspidatum extract, 3 parts of Amyda sinensis leaf extract, and 1 part of Rosa rugosa fruit extract by weight, mix them well to obtain the plant extract composition.
[0103] Example 8
[0104] Take the four plant extracts prepared in Preparation Example 1, and take 1 part of rosemary extract, 1 part of Polygonum cuspidatum extract, 4 parts of Amyda sinensis leaf extract, and 1 part of Rosa rugosa fruit extract by weight. Mix them well to obtain the plant extract composition.
[0105] Example 9
[0106] Take the four plant extracts prepared in Preparation Example 1, and take 1 part of rosemary extract, 1 part of Polygonum cuspidatum extract, 1 part of Amyda sinensis leaf extract, and 3 parts of Rosa rugosa fruit extract by weight. Mix them well to obtain the plant extract composition.
[0107] Example 10
[0108] Take the four plant extracts prepared in Preparation Example 1, and take 1 part of rosemary extract, 1 part of Polygonum cuspidatum extract, 1 part of Amygdalus leaf extract, and 5 parts of Rosa rugosa fruit extract by weight, mix them well to obtain the plant extract composition.
[0109] Example 11
[0110] Take the four plant extracts prepared in Preparation Example 1, and take 1 part of rosemary extract, 1 part of Polygonum cuspidatum extract, 1 part of Amygdalus leaf extract, and 7 parts of Rosa rugosa fruit extract by weight, mix them well to obtain the plant extract composition.
[0111] Example 12
[0112] Take the four plant extracts prepared in Preparation Example 1, and take 1 part of rosemary extract, 1 part of Polygonum cuspidatum extract, 1 part of Amyda sinensis leaf extract, and 9 parts of Rosa rugosa fruit extract by weight. Mix them well to obtain the plant extract composition.
[0113] Example 13
[0114] Dried rosemary leaves, Polygonum cuspidatum rhizome, Ampelopsis japonica leaves, and Rosa rugosa fruit were mixed and pulverized. The pulverized mixture was first mixed with 675 mL of 95% ethanol and extracted using ultrasound at 380 W for 60 min. After extraction, solid-liquid separation was performed, and extract 1 was collected. The solid was then mixed with 675 mL of 80% ethanol and extracted using ultrasound at 380 W for 60 min. After extraction, solid-liquid separation was performed, and extract 2 was collected. The solid was then mixed with 675 mL of 65% ethanol and extracted using ultrasound at 380 W. Extraction was carried out for 60 min; after extraction, solid and liquid were separated, and extract 3 was collected. The solid was then mixed with 675 mL of 50% ethanol and extracted under ultrasonic power of 380 W for 60 min; after extraction, solid and liquid were separated, and extract 4 was collected. The solid was then mixed with 675 mL of 35% ethanol and extracted under ultrasonic power of 380 W for 60 min; after extraction, solid and liquid were separated, and extract 5 was collected. Extracts 1, 2, 3, 4 and 5 were mixed and concentrated under reduced pressure until dried to obtain the plant extract composition.
[0115] Example 14
[0116] The plant extract composition used in Example 1 is the same as the one used in the acne cream, with the raw material content percentages shown in Table 2:
[0117] Table 2. Percentage of Ingredients in Acne Cream
[0118]
[0119]
[0120] The preparation method for acne cream is as follows:
[0121] (1) Add propylene glycol, jojoba seed oil, butter from Butyrospermum Parkii fruit, hydrogenated polydecene, cetearyl alcohol, petrolatum, polydimethylsiloxane, lauric acid / myristic acid / palmitic acid / glyceryl stearate, hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, arachidonic acid, sodium lauryl sulfate, behenyl alcohol, C20-22 phosphate ester, polyisobutylene, C20-22 alcohol, cetearyl glucoside, arachidonic acid glucoside, PEG-7 trimethylolpropionic acid coco ether, sorbitan isostearate, sodium sulfate, and C12-16 alcohol to an oil pan, mix and heat to 80°C, stir until completely dissolved, and keep warm for 15 minutes to obtain oil phase A;
[0122] (2) Dissolve sodium hyaluronate completely in distilled water by heating to 80°C to obtain aqueous phase B;
[0123] (3) Pour phase A into phase B, heat and stir at 75-80℃ until uniform, then stir and cool down to 45℃; add the mixture of plant extract composition, ascorbic acid, carnosine, fructose, butylene glycol, phosphatidylcholine, ceramide NP, polyglycerol-10 oleate, sodium stearoyl glutamate, glyceryl caprylate and p-hydroxyacetophenone, stir at 1200r until uniform, and keep for 10 minutes;
[0124] (4) Add the preservative phenoxyethanol to (3), stir continuously at 1200r for 5 minutes, continue stirring and cool to 30°C, filter and discharge to obtain an acne cream containing a plant extract composition with acne-removing effects.
[0125] Comparative Example 1
[0126] The only difference from Example 1 is that the plant extract composition does not contain rosemary extract.
[0127] Comparative Example 2
[0128] The only difference from Example 1 is that the plant extract composition does not contain Polygonum cuspidatum extract.
[0129] Comparative Example 3
[0130] The only difference from Example 1 is that the plant extract composition does not contain Ampelopsis japonica leaf extract.
[0131] Comparative Example 4
[0132] The only difference from Example 1 is that the plant extract composition does not contain prickly pear fruit extract.
[0133] Example of effect 1
[0134] In vitro experiments on antibacterial, anti-inflammatory and antioxidant effects
[0135] 1. In vitro experiment against Propionibacterium acnes
[0136] The plant extract compositions prepared in Examples 1-13 and Comparative Examples 1-4 were subjected to in vitro antibacterial assays against Propionibacterium acnes.
[0137] 1.1 Minimum Antimicrobial Concentration (MIC) Determination Method
[0138] Well plates were prepared using the broth microdilution method. Propionibacterium acnes was inoculated into Mueller-Hinton broth (MHB) and cultured. Plant extract compositions were dissolved in DMSO and tested at final concentrations ranging from 128 to 0.0625 μg / mL. Bacterial cultures (100 μL) of each strain were diluted at 5 × 10⁻⁶ microdiluted solutions.5 An inoculum of CFU / mL was added to the wells of the plate. In the first row, an additional 98 μL of bacterial suspension and 2 μL of each plant extract composition sample stock solution were added and mixed. Then, 100 μL of each stock solution was transferred sequentially to the second row to make a final volume of 100 μL. After anaerobic incubation at 37°C for 48 hours, the lowest concentration at which no visible bacterial growth was observed was determined as the minimum antibacterial concentration (MIC). Rifampin was used as a positive control.
[0139] Test strains: Propionibacterium acnes (ATCC1182) were all provided by the China National Institutes for Food and Drug Control.
[0140] 1.2 Experimental Results
[0141] Examples 1-13 and Comparative Examples 1-4 were used to conduct in vitro antibacterial efficacy experiments against Propionibacterium acnes. The results are shown in Table 3. As shown in Table 3, Examples 1-13 of the present invention have significant inhibitory effects on Propionibacterium acnes. Among them, Example 1 has the most significant antibacterial effect. Compared with Example 1, the antibacterial activity of Comparative Examples 1-4 is significantly reduced, indicating that the four extracts can synergistically enhance each other and increase the activity. The changes in the composition of Examples 1-13 show that when the proportions of rosemary extract, Ampelopsis japonica leaf extract, and Rosa rugosa fruit extract exceed a certain limit, the activity does not increase and may even decrease. When the proportions of rosemary extract exceed 9 parts, Ampelopsis japonica leaf extract exceed 3 parts, and Rosa rugosa fruit extract exceed 5 parts, the activity no longer increases or decreases.
[0142] Table 3. Results of minimum antibacterial concentration (MIC) determination (n=3, X±SD)
[0143]
[0144]
[0145] 2. Anti-inflammatory activity test
[0146] The anti-inflammatory activity of the plant extract compositions prepared in Examples 1-13 and Comparative Examples 1-4 was tested.
[0147] 2.1. Assay for the anti-inflammatory activity of LPS-induced RAW264.7 cell model
[0148] Cell line: RAW264.7 macrophages, purchased from the cell resource platform of Peking Union Medical College.
[0149] Cell culture: Cells were cultured in a constant temperature cell culture incubator at 37°C and 5% CO2 under the following conditions: high glucose DMEM complete culture medium containing 15% fetal bovine serum (containing 1% penicillin-streptomycin mixture).
[0150] CCK-8 cytotoxic activity assay: Add 8 × 10⁸ g of the solution to a 96-well plate. 3 RAW264.7 cells in the logarithmic growth phase were cultured overnight in a 5% CO2 incubator at 37°C with 100 μL / well. Different concentrations of sample were added to different experimental groups, or an equal volume of culture medium was added to the blank control group for 24 h, with each group having three replicates. Then, following the instructions of the CCK-8 kit, 10 μL of CCK-8 reagent was added directly to each well, and after incubation at 37°C for 2 hours, the OD value was measured at 450 nm using a microplate reader.
[0151] Cell viability (%) = mean of drug-treated group / blank group × 100%.
[0152] NO content determination: Add 8×10⁻⁶ to a 96-well plate. 3 RAW264.7 cells in the logarithmic growth phase were incubated overnight at 37°C with 5% CO2. Different concentrations of sample were added to the experimental groups, while the blank and model groups were added with equal volumes of culture medium. Pretreatment was performed for 2 hours, with three replicates per group. LPS solution (1 μg / mL) was then added, and the cells were incubated at 37°C with 5% CO2 for 24 hours. After incubation, the NO content in the supernatant was measured according to the NO reagent kit instructions. 50 μL of the supernatant was collected and added to a 96-well plate, followed by 50 μL of Griess Reagent I and 50 μL of Griess Reagent II. The plate was shaken at room temperature in the dark for 5 minutes, and the OD value was measured at 540 nm using a microplate reader. A standard curve of absorbance versus NaNO2 was established, and the NO content was calculated based on the standard curve. Hydrocortisone (20 μg / mL) was used as the positive control.
[0153] 2.2 Experimental Results
[0154] Firstly, cytotoxicity experiments were conducted, and no cytotoxicity was found in any of the compositions from the examples and comparative examples. Subsequently, anti-inflammatory effects were tested using Examples 1-13 and Comparative Examples 1-4 as samples, and the results are shown in Table 4. The results indicate that in the LPS-stimulated RAW264.7 cell inflammation model, Examples 4-13 significantly reduced NO release compared to the model group, exhibiting a concentration-dependent effect. Example 4 showed the most significant anti-inflammatory effect. Compared to Example 1, Comparative Examples 1-4 showed a significantly weaker inhibitory effect on NO release, indicating that the compounded compositions can significantly improve the inhibition rate of NO release and exhibit a strong anti-inflammatory effect.
[0155] Table 4. NO release levels in the LPS-stimulated RAW264.7 cell model (n=3, X±SD, μM)
[0156]
[0157]
[0158] Note: ### P<0.001 vs. blank group; * P<0.05, ** P<0.01, *** P<0.001 vs. model group
[0159] 3. Antioxidant activity assay
[0160] The antioxidant activity of the plant extract compositions prepared in Examples 1-13 and Comparative Examples 1-4 was tested.
[0161] 3.1. Experimental Methods for Antioxidant Determination
[0162] (1) Test experiment on DPPH free radical scavenging ability
[0163] Accurately weigh 9.858 mg DPPH, dissolve it in 95% ethanol solution, and dilute to a final volume of 250 mL in a brown volumetric flask to prepare a DPPH free radical solution with a concentration of 0.1 mmol / L. Prepare fresh before use. Mix 150 μL of the DPPH free radical solution and 150 μL of the 100 μg / mL sample solution in an EP tube. Use the same concentration of vitamin C as a positive control and 95% ethanol solution as a blank control. Incubate at 25°C in the dark for 30 min. Then, take 150 μL of each reaction solution and place it in a 96-well plate for measurement. Set up three wells for each reaction solution of different concentrations. Measure the absorbance of the reaction mixture at 517 nm using a microplate reader. The final absorbance is the average value. The DPPH free radical scavenging rate is calculated as follows:
[0164] DPPH removal rate = [1 - A1 / A0] × 100
[0165] A1—Absorbance of the sample reaction solution
[0166] A0 – Absorbance of blank control
[0167] (2) ABTS + Test methods for clearing ability
[0168] Weigh ABTS + Potassium persulfate powder was prepared with room temperature ultrapure water to a concentration of 7 mmol / L. + ABTS is obtained by mixing 40 mL of a 1:1 solution of potassium persulfate and 2.45 mmol / L potassium persulfate, and then placing the mixture in a constant temperature incubator (23℃) in the dark for 16 hours. + Base liquid. ABTS + Preparation of working solution: Take ABTS +10 mL of base solution was diluted with ultrapure water, and the absorbance of the diluted solution was measured at a wavelength of 734 nm. ABTS samples with absorbance in the range of 0.70 ± 0.02 were finally obtained. + Working solution. Take 40 μL of the sample solution with a concentration of 100 μg / mL and 200 μL of ABTS. + The working solution was poured into a 96-well plate and gently mixed. Three wells were set up for each sample solution of different concentrations. The plates were incubated at 23°C in the dark for 6 minutes. The OD value of the incubation solution at 734 nm was measured using a microplate reader, and the average OD value was taken. Vitamin C was used as a positive control, and 95% ethanol solution was used as a blank control. The ABTS cationic radical scavenging rate was calculated as follows:
[0169] ABTS + Clearance rate = [1 - A1 / A0] × 100
[0170] A1—Absorbance of the sample reaction solution
[0171] A0 – Absorbance of blank control
[0172] (3) Test experiment on the total antioxidant capacity of FRAP
[0173] Determination of the standard curve: Following the kit instructions, weigh 27.8 mg of FeSO4·7H2O solid, dissolve it in distilled water, and finally bring the volume to 1 mL to obtain a 100 mM FeSO4 solution. Using a serial dilution method, the 100 mM FeSO4·7H2O solution was diluted to obtain six standard solutions with concentrations of 0.3, 0.6, 0.9, 1.2, 1.5, and 1.8 mM. Take 5 μL of each concentration of standard solution and 180 μL of FRAP working solution into a 96-well plate, gently mix, and assign three wells to each concentration of standard solution. Incubate at 37℃ for 3-5 min, and measure the OD value of the incubation solution at 593 nm using a microplate reader to plot the standard curve.
[0174] Total antioxidant capacity determination: Take 5 μL of sample solution with a concentration of 100 μg / mL and 180 μL of FRAP working solution into a 96-well plate, shake gently, and set up 3 wells for sample solutions of different concentrations respectively. Incubate at 37℃ for 3-5 min, and measure the OD value of the incubation solution at a wavelength of 593 nm using a microplate reader. Distilled water is used as a blank control. The total antioxidant capacity is calculated according to the standard curve and expressed as the concentration of FeSO4 standard solution.
[0175] 3.2. Experimental Results
[0176] Antioxidant effects were tested using Examples 1-13 and Comparative Examples 1-4 as samples, and the results are shown in Table 5. The results indicate that ABTS... +In the free radical scavenging experiment and the FRAP total antioxidant capacity test, Examples 1-13 showed significant antioxidant effects, with Example 1 showing the most significant effect. Comparative Examples 1-4, compared to Example 4, exhibited significantly weaker antioxidant capacity, indicating that the plant extract composition, after scientific formulation, demonstrated a significant antioxidant enhancement effect.
[0177] Table 5. Results of antioxidant experiments (n=3, X±SD)
[0178]
[0179] Test Case 1: Acne-removing efficacy and human trial on sensitive skin
[0180] The acne cream prepared in Example 14 was subjected to acne-removing efficacy and human trials on sensitive skin (testing unit: PONY Testing Group Co., Ltd., test results are as follows). Figure 3 (As shown).
[0181] Thirty participants with sensitive facial skin and acne were recruited and screened. They used the product regularly and underwent subjective evaluation and instrumental testing at set time points. The product was evaluated by assessing the percentage of red area, skin color (a*), and acne count at the test sites before product use and at 7, 14, and 28 days after product use. The evaluation aimed to assess whether the product reduced or slowed down acne occurrence, its skin recovery function, and its acne-reducing efficacy and suitability for sensitive skin.
[0182] Test results are as follows Figure 2 As shown, by Figure 2 It can be seen that after 7 days of use, the percentage of red area decreased significantly (p<0.05), and the facial condition improved significantly. After 14 and 28 days of use, the percentage of red area, the number of pimples, and the a* value of skin color decreased significantly (P<0.05), indicating that it helps to reduce and alleviate the occurrence of pimples and helps the skin recover after pimples occur. The product has the effect of removing acne.
[0183] The results of the sensitive skin test are shown in Table 6. No adverse events occurred in the sensitive skin subjects after 7 days, 14 days and 28 days of use, indicating that the product is suitable for sensitive skin.
[0184] Table 6 Adverse Skin Reactions in Human Use Trials
[0185]
[0186] Note: No adverse events were observed during this test.
[0187] Test Example 2: Acute Eye Irritation Test (Testing Unit: PONY Testing Group Co., Ltd., Test Report as follows) Figure 4 (As shown)
[0188] The acne cream prepared in Example 14 was used in an acute eye irritation test. The test animals were rabbits, specifically Japanese White rabbits, grade: ordinary; number: 3 rabbits, weighing 2-3 kg. 0.1 mL of the test substance was instilled into the conjunctival sac under one eyelid of each rabbit, and the upper and lower eyelids were passively closed for 1 second to prevent loss of the test substance. The eyes were not rinsed within 24 hours. Eye conditions were observed at 1 hour, 24 hours, 48 hours, and 72 hours, and scored according to the "Cosmetic Safety Technical Specifications" (2015 edition).
[0189] The experimental results are shown in Table 7. The results show that the acne cream did not irritate the eyes of rabbits without rinsing.
[0190] Table 7 Results of the acute eye irritation test on rabbits by the test substances
[0191]
[0192]
[0193] Note: The mean is rounded to two decimal places.
[0194] Test Case 3: Repeated Skin Irritation Test (Testing Unit: PONY Testing Group Co., Ltd., Test Report as follows) Figure 4 (As shown)
[0195] The acne cream prepared in Example 14 was used in multiple skin irritation tests. The test animals were rabbits, specifically Japanese White rabbits, grade: ordinary; number: 3, weighing 2-3 kg. 24 hours before the test, the hair on both sides of the spine on the back of the test animals was trimmed, taking care not to damage the epidermis; the trimmed area was 3cm x 3cm on each side. 0.5mL of the test product was applied directly to one side of the skin, covering an area of 2.5cm x 2.5cm, once daily for 14 consecutive days, and scored according to the "Cosmetic Safety Technical Specifications" (2015 edition).
[0196] The test results are shown in Table 8. The results show that the acne cream prepared in Example 14 did not irritate the skin of rabbits after repeated use.
[0197] Table 8 Results of repeated skin irritation tests on rabbits by the test substances
[0198]
[0199] Note: The mean of the integrals is rounded to two decimal places.
[0200] Test Example 4: Physicochemical Testing (Testing Unit: PONY Testing Group Co., Ltd., Test Report as follows) Figure 5 , Figure 6 (As shown)
[0201] The acne cream prepared in Example 14 was subjected to physicochemical testing. Acrylamide, phenol, diethylene glycol and pesticide residues were tested according to the "Cosmetic Safety Technical Specifications".
[0202] The test results are shown in Table 9. The results indicate that the acrylamide level is <0.005 mg / kg, phenol and diethylene glycol are not detected, and pesticide residues are not detected, which meets the requirements of the cosmetic safety technical specifications.
[0203] Table 9. Physicochemical Test Results
[0204]
[0205] Example 5: Microbial testing (Testing unit: PONY Testing Group Co., Ltd., test report as follows) Figure 7 (As shown)
[0206] The acne cream prepared in Example 14 was subjected to microbial testing according to the "Cosmetic Safety Technical Specifications" (2015 edition), and the test results are shown in Table 10.
[0207] Table 10 Microbiological Detection Results
[0208]
[0209] The results showed that the total number of bacterial species in the acne cream obtained in Example 14 was <10, the total number of molds and yeasts was <10, and thermotolerant Escherichia coli, Staphylococcus aureus, and Pseudomonas aeruginosa were not detected. It meets the requirements of the "Cosmetic Safety Technical Specifications" (2015 edition).
[0210] Example 6: Heavy Metal Testing (Testing Unit: PONY Testing Group Co., Ltd., Test Report as follows) Figure 7 (As shown)
[0211] The acne cream prepared in Example 14 was tested for heavy metals according to the "Cosmetic Safety Technical Specifications" (2015 edition), and the test results are shown in Table 11.
[0212] Table 11 Heavy Metal Detection Results
[0213]
[0214] The results showed that the levels of heavy metals mercury, lead, arsenic, cadmium, and dioxane in the acne cream met the requirements of the "Cosmetic Safety Technical Specifications" (2015 edition).
[0215] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.
Claims
1. An acne cream, characterized in that, It is composed of the following components in the indicated mass fractions: propylene glycol 5-10%, jojoba seed oil 2-8%, shea butter 1-10%, hydrogenated polydecene 1-10%, cetearyl alcohol 1-7%, petrolatum 1-6%, polydimethylsiloxane 1-5%, lauric acid / myristic acid / palmitic acid / glyceryl stearate esters 0.1-1.5%, hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer 0.1-0.6%, peanut alcohol 0.1-2%, sodium lauryl sulfate 0.1-2.5%, plant extract composition 0.04-19%, sodium hyaluronate 0.1-1%, phenoxyethanol 0.1-0.9%, and ascorbic acid 0.1-3%. 8%, behenol 0.1–4.5%, C20-22 alcohol phosphate 0.1–2.9%, polyisobutylene 0.1–10%, C20-22 alcohol 0.1–3.1%, cetearyl glucoside 0.1–5.2%, carnosine 0.1–5%, arachidonic acid glucoside 0.1–2.5%, PEG-7 trimethylolpropionic acid ether 0.01–0.3%, sorbitan isostearate 0.01–5.7%, sodium sulfate 0.01–3%, C12–16 alcohol 0.001–4.3%, fructose 0.01–1.9%, butylene glycol 0.01–5.6%, phosphatidylcholine 0.01–3.4%, ceramide NP 0.001–1.3%, polyglycerol-10 oleate 0.001–1.8%, sodium stearoyl glutamate 0.001–1.5%, glyceryl caprylate 0.0001–2.2%, p-hydroxyacetophenone 0.0001–0.6%, balance being water.
2. The acne cream according to claim 1, characterized in that, The plant extract composition comprises the following components in parts by weight: 0.01-9 parts rosemary extract, 0.01-2 parts Polygonum cuspidatum extract, 0.01-3 parts Ampelopsis japonica leaf extract, and 0.01-5 parts Rosa rugosa fruit extract. The method for preparing the rosemary extract includes: gradient extraction of rosemary with ethanol, wherein the ratio of rosemary to ethanol is 1:10-20 (g / mL); the gradient extraction is performed sequentially with ethanol at volume concentrations of 100%, 85%, and 70%. The preparation method of the Polygonum cuspidatum extract includes: gradient extraction of Polygonum cuspidatum with ethanol, wherein the ratio of Polygonum cuspidatum to ethanol is 1:10-20 (g / mL); the gradient extraction is performed sequentially with ethanol at volume concentrations of 90%, 80%, and 70%. The preparation method of the Aeonium phalloides leaf extract includes: gradient extraction of Aeonium phalloides leaves with ethanol, wherein the ratio of Aeonium phalloides leaves to ethanol is 1:10-20 (g / mL); the gradient extraction is performed sequentially with ethanol at volume concentrations of 95%, 85%, and 75%. The preparation method of the prickly pear fruit extract includes: extracting the prickly pear fruit with ethanol, wherein the ratio of prickly pear fruit to ethanol is 1:10-15 (g / mL); the gradient extraction is performed sequentially with ethanol at volume concentrations of 50%, 35%, and 20%.
3. The acne cream according to claim 1, characterized in that, The method for preparing the plant extract composition includes mixing and pulverizing rosemary, Japanese knotweed, Amaryllis leaves and prickly pear fruit to obtain a mixture, and then performing gradient extraction on the mixture to obtain the plant extract composition. The mass ratio of rosemary, Japanese knotweed, Amaryllis leaves, and prickly pear fruit is 1:1:1:
1.
4. The acne cream according to claim 3, characterized in that, The gradient extraction includes: sequentially extracting the mixture with ethanol at volume concentrations of 95%, 80%, 65%, 50%, and 35%; the material-to-liquid ratio of the mixture to ethanol is 1:15–20 (g / mL).
5. The method for preparing the acne cream according to any one of claims 1 to 4, characterized in that, Includes the following steps: (1) Propylene glycol, jojoba seed oil, shea butter, hydrogenated polydecene, cetearyl alcohol, petrolatum, polydimethylsiloxane, lauric acid / myristic acid / palmitic acid / glyceryl stearate, hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer, arachidonic acid, sodium lauryl sulfate, behenyl alcohol, C20-22 phosphate ester, polyisobutylene, C20-22 alcohol, cetearyl glucoside, arachidonic acid glucoside, PEG-7 trimethylolpropionic acid coco ether, sorbitan isostearate, sodium sulfate and C12-16 alcohol are mixed to obtain oil phase A; (2) Sodium hyaluronate and water are mixed to obtain aqueous phase B; (3) After mixing oil phase A and water phase B, add plant extract composition, ascorbic acid, carnosine, fructose, butylene glycol, phosphatidylcholine, ceramide NP, polyglycerol-10 oleate, sodium stearoyl glutamate, glyceryl caprylate, p-hydroxyacetophenone and phenoxyethanol and stir evenly to obtain acne cream.
6. The preparation method according to claim 5, characterized in that, The mixing temperature in step (1) is 75-80℃ and the time is 10-15 min.
7. The preparation method according to claim 5, characterized in that, The mixing temperature in step (2) is 75-80℃.
8. The preparation method according to claim 5, characterized in that, Step (3) The oil phase A and water phase B are mixed at a temperature of 75-80°C. After mixing evenly, the temperature is lowered to 45-50°C, and other components are added.
9. The preparation method according to claim 5, characterized in that, Step (3) The stirring speed is 1000-1200 r and the time is 10-15 min.
10. The use of the acne cream according to any one of claims 1 to 4 in the preparation of facial care, body care, hair care or oral care products.